# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cuno3tha-f
_database_code_depnum_ccdc_archive 'CCDC 1901777'
loop_
_audit_author_name
_audit_author_address
MICHAUD
;UNIVERSITE DE BRETAGNE OCCIDENTALE
France
;
_audit_update_record             
;
2019-03-07 deposited with the CCDC.	2019-05-17 downloaded from the CCDC.
;

_audit_creation_date             2016-12-05T11:40:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
;
        C21 H22 Cu N6 O6 S3, 4(H2 O)
;
_chemical_formula_sum            'C21 H30 Cu N6 O10 S3'
_chemical_formula_weight         686.23

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  -P1
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9546(4)
_cell_length_b                   10.9939(5)
_cell_length_c                   14.0477(6)
_cell_angle_alpha                85.134(4)
_cell_angle_beta                 86.799(3)
_cell_angle_gamma                81.534(4)
_cell_volume                     1361.62(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6428
_cell_measurement_theta_min      3.72
_cell_measurement_theta_max      27.468

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       'prism (fragment), axis [0 0 1]'
_exptl_crystal_colour            'light green'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             710
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.05
0 1 0 0.02
1 0 0 0.025
-1 0 0 0.025
0 0 -1 0.17
0 1 1 0.02
1 1 1 0.025
-1 -1 -1 0.11
3 5 2 0.01
1 3 1 0.005
-3 -2 5 0.085

_exptl_crystal_recrystallization_method 
'from aqueous solution at room temperature,by slow evaporation of water'
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
        (compiled Aug  4 2014,14:34:23)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.5694
_exptl_absorpt_correction_T_max  0.9471

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_orient_matrix_ub_11      -0.0788548
_diffrn_orient_matrix_ub_12      0.0207305
_diffrn_orient_matrix_ub_13      0.0027687
_diffrn_orient_matrix_ub_21      -0.0133498
_diffrn_orient_matrix_ub_22      -0.0532092
_diffrn_orient_matrix_ub_23      -0.0215798
_diffrn_orient_matrix_ub_31      -0.0054252
_diffrn_orient_matrix_ub_32      -0.0319296
_diffrn_orient_matrix_ub_33      0.0458213
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0951
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_number            16901
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.23
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             5560
_reflns_number_gt                4356
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
        (compiled Aug  4 2014,14:34:23)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
        (compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
        (compiled Aug  4 2014,14:34:23)
;
_computing_structure_solution    'SIR-92 (Altomare et al., 1992)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
        ORTEP3 for Windows (Farrugia, 1997)
        MERCURY  (Bruno et al., 2002)
;
_computing_publication_material  
;
        WinGX (Farrugia, 1999)
        PLATON (Spek, 1990-2003)
        enCIFer (Allen et al., 2004)
;

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0547P)²+0.1381P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5560
_refine_ls_number_parameters     397
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.063
_refine_ls_R_factor_gt           0.0468
_refine_ls_wR_factor_ref         0.1273
_refine_ls_wR_factor_gt          0.1143
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_restrained_S_all      1.03
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.08

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0794(4) 0.0849(3) 0.2646(2) 0.0399(8) Uani 1 1 d D . .
H1A H -0.0259 0.1107 0.2825 0.048 Uiso 1 1 calc R . .
H1B H 0.0988 -0.0044 0.2723 0.048 Uiso 1 1 calc R . .
C2 C 0.1104(4) 0.1283(3) 0.1606(2) 0.0390(8) Uani 1 1 d . . .
H2A H 0.1961 0.0754 0.134 0.047 Uiso 1 1 calc R . .
H2B H 0.0232 0.124 0.1237 0.047 Uiso 1 1 calc R . .
C3 C 0.0057(4) 0.3464(3) 0.1679(3) 0.0436(8) Uani 1 1 d . . .
H3A H -0.0772 0.3032 0.1919 0.052 Uiso 1 1 calc R . .
H3B H -0.0208 0.3881 0.1062 0.052 Uiso 1 1 calc R . .
C4 C 0.0260(4) 0.4433(3) 0.2374(3) 0.0404(8) Uani 1 1 d . . .
H4A H 0.0875 0.5018 0.2059 0.048 Uiso 1 1 calc R . .
H4B H -0.0719 0.4883 0.2545 0.048 Uiso 1 1 calc R . .
C5 C 0.0060(4) 0.3119(3) 0.3871(3) 0.0407(8) Uani 1 1 d . . .
H5A H -0.083 0.3004 0.3545 0.049 Uiso 1 1 calc R . .
H5B H -0.0272 0.3551 0.4436 0.049 Uiso 1 1 calc R . .
C6 C 0.0951(4) 0.1862(3) 0.4168(2) 0.0408(8) Uani 1 1 d D . .
H6A H 0.1658 0.1945 0.4649 0.049 Uiso 1 1 calc R . .
H6B H 0.027 0.1299 0.4433 0.049 Uiso 1 1 calc R . .
C7 C 0.3216(3) 0.0558(3) 0.3519(2) 0.0340(7) Uani 1 1 d D . .
H7A H 0.2974 -0.0214 0.3832 0.041 Uiso 1 1 calc R . .
H7B H 0.3757 0.0942 0.3963 0.041 Uiso 1 1 calc R . .
C8 C 0.4217(3) 0.0296(3) 0.2648(2) 0.0301(7) Uani 1 1 d . . .
C9 C 0.5728(4) -0.0649(3) 0.1374(3) 0.0412(8) Uani 1 1 d . . .
H9 H 0.6245 -0.1142 0.0921 0.049 Uiso 1 1 calc R . .
C10 C 0.5865(3) 0.0554(3) 0.1438(2) 0.0313(7) Uani 1 1 d . . .
C11 C 0.6943(3) 0.1273(3) 0.0844(2) 0.0341(7) Uani 1 1 d . . .
C12 C 0.2403(4) 0.2880(3) 0.0736(2) 0.0371(7) Uani 1 1 d . . .
H12A H 0.1815 0.305 0.0169 0.044 Uiso 1 1 calc R . .
H12B H 0.3183 0.2188 0.063 0.044 Uiso 1 1 calc R . .
C13 C 0.3120(3) 0.3983(3) 0.0897(2) 0.0327(7) Uani 1 1 d . . .
C14 C 0.3835(4) 0.6026(3) 0.0871(2) 0.0414(8) Uani 1 1 d . . .
H14 H 0.3975 0.685 0.0787 0.05 Uiso 1 1 calc R . .
C15 C 0.4586(3) 0.5171(3) 0.1490(2) 0.0302(7) Uani 1 1 d . . .
C16 C 0.5879(3) 0.5310(3) 0.2088(2) 0.0330(7) Uani 1 1 d . . .
C17 C 0.1711(4) 0.4710(3) 0.3735(3) 0.0408(8) Uani 1 1 d . . .
H17A H 0.0976 0.5151 0.4163 0.049 Uiso 1 1 calc R . .
H17B H 0.2082 0.5311 0.327 0.049 Uiso 1 1 calc R . .
C18 C 0.3002(4) 0.4047(3) 0.4297(2) 0.0376(7) Uani 1 1 d . . .
C19 C 0.4820(4) 0.3294(4) 0.5494(2) 0.0477(9) Uani 1 1 d . . .
H19 H 0.5403 0.3075 0.6026 0.057 Uiso 1 1 calc R . .
C20 C 0.5202(4) 0.2922(3) 0.4603(2) 0.0362(7) Uani 1 1 d . . .
C21 C 0.6619(4) 0.2124(3) 0.4310(2) 0.0371(7) Uani 1 1 d . . .
N1 N 0.1786(3) 0.1380(2) 0.32882(18) 0.0304(6) Uani 1 1 d D . .
N2 N 0.1427(3) 0.2559(2) 0.15515(18) 0.0328(6) Uani 1 1 d . . .
N3 N 0.0979(3) 0.3858(2) 0.32413(19) 0.0342(6) Uani 1 1 d . . .
N4 N 0.4992(3) 0.1092(2) 0.21685(16) 0.0275(5) Uani 1 1 d . . .
N5 N 0.4160(3) 0.4011(2) 0.15119(16) 0.0270(5) Uani 1 1 d . . .
N6 N 0.4151(3) 0.3342(2) 0.39249(17) 0.0324(6) Uani 1 1 d . . .
O1 O 0.7011(2) 0.2327(2) 0.10926(16) 0.0392(5) Uani 1 1 d . . .
O2 O 0.7658(3) 0.0755(2) 0.01653(18) 0.0538(7) Uani 1 1 d . . .
O3 O 0.6427(2) 0.4328(2) 0.25705(15) 0.0358(5) Uani 1 1 d . . .
O4 O 0.6328(3) 0.6322(2) 0.2067(2) 0.0520(7) Uani 1 1 d . . .
O5 O 0.6829(2) 0.1928(2) 0.34282(16) 0.0370(5) Uani 1 1 d . . .
O6 O 0.7527(3) 0.1686(3) 0.49304(17) 0.0559(7) Uani 1 1 d . . .
S1 S 0.44880(10) -0.11339(8) 0.22306(7) 0.0440(2) Uani 1 1 d . . .
S2 S 0.26059(10) 0.53789(8) 0.02706(6) 0.0438(2) Uani 1 1 d . . .
S3 S 0.31222(12) 0.42201(10) 0.54944(6) 0.0533(3) Uani 1 1 d . . .
Cu Cu 0.55071(4) 0.28198(3) 0.24339(2) 0.02902(13) Uani 1 1 d . . .
H1N H 0.203(3) 0.2041(18) 0.2945(15) 0.035 Uiso 1 1 d D . .
O7 O 0.0307(4) 0.1429(3) 0.9213(3) 0.0714(9) Uani 1 1 d D . .
H7V H -0.062(2) 0.136(5) 0.928(4) 0.107 Uiso 1 1 d D . .
H7W H 0.080(5) 0.074(3) 0.939(4) 0.107 Uiso 1 1 d D . .
O8 O 0.1252(4) 0.2431(3) 0.7433(2) 0.0677(8) Uani 1 1 d D . .
H8V H 0.090(5) 0.224(5) 0.8003(19) 0.101 Uiso 1 1 d D . .
H8W H 0.184(5) 0.292(4) 0.754(4) 0.101 Uiso 1 1 d D . .
O9 O -0.1663(4) 0.2281(4) 0.6706(3) 0.0844(10) Uani 1 1 d D . .
H9V H -0.073(3) 0.244(6) 0.676(4) 0.127 Uiso 1 1 d D . .
H9W H -0.168(6) 0.226(6) 0.6076(16) 0.127 Uiso 1 1 d D . .
O10 O 0.2794(6) 0.0829(4) 0.6078(3) 0.1058(14) Uani 1 1 d D . .
H10V H 0.209(6) 0.120(5) 0.646(4) 0.159 Uiso 1 1 d D . .
H10W H 0.263(8) 0.008(2) 0.621(5) 0.159 Uiso 1 1 d D . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.509(4) . ?
C1 C2 1.521(5) . ?
C1 H1A 0.97 . ?
C1 H1B 0.97 . ?
C2 N2 1.468(4) . ?
C2 H2A 0.97 . ?
C2 H2B 0.97 . ?
C3 N2 1.474(4) . ?
C3 C4 1.541(5) . ?
C3 H3A 0.97 . ?
C3 H3B 0.97 . ?
C4 N3 1.462(4) . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
C5 N3 1.453(4) . ?
C5 C6 1.528(5) . ?
C5 H5A 0.97 . ?
C5 H5B 0.97 . ?
C6 N1 1.503(4) . ?
C6 H6A 0.97 . ?
C6 H6B 0.97 . ?
C7 N1 1.489(4) . ?
C7 C8 1.499(4) . ?
C7 H7A 0.97 . ?
C7 H7B 0.97 . ?
C8 N4 1.314(4) . ?
C8 S1 1.703(3) . ?
C9 C10 1.356(4) . ?
C9 S1 1.698(4) . ?
C9 H9 0.93 . ?
C10 N4 1.375(4) . ?
C10 C11 1.509(4) . ?
C11 O2 1.249(4) . ?
C11 O1 1.249(4) . ?
C12 N2 1.453(4) . ?
C12 C13 1.492(4) . ?
C12 H12A 0.97 . ?
C12 H12B 0.97 . ?
C13 N5 1.310(3) . ?
C13 S2 1.717(3) . ?
C14 C15 1.354(4) . ?
C14 S2 1.693(3) . ?
C14 H14 0.93 . ?
C15 N5 1.382(4) . ?
C15 C16 1.501(4) . ?
C16 O4 1.235(4) . ?
C16 O3 1.274(4) . ?
C17 N3 1.460(4) . ?
C17 C18 1.499(5) . ?
C17 H17A 0.97 . ?
C17 H17B 0.97 . ?
C18 N6 1.307(4) . ?
C18 S3 1.719(3) . ?
C19 C20 1.359(5) . ?
C19 S3 1.701(4) . ?
C19 H19 0.93 . ?
C20 N6 1.380(4) . ?
C20 C21 1.491(5) . ?
C21 O6 1.243(4) . ?
C21 O5 1.274(4) . ?
N1 H1N 0.885(18) . ?
N4 Cu 2.087(2) . ?
N5 Cu 2.066(2) . ?
N6 Cu 2.430(2) . ?
O1 Cu 2.309(2) . ?
O3 Cu 1.984(2) . ?
O5 Cu 1.981(2) . ?
O7 H7V 0.844(19) . ?
O7 H7W 0.843(19) . ?
O8 H8V 0.865(19) . ?
O8 H8W 0.837(19) . ?
O9 H9V 0.888(19) . ?
O9 H9W 0.889(19) . ?
O10 H10V 0.88(2) . ?
O10 H10W 0.86(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 110.4(2) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C1 109.3(3) . . ?
N2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
N2 C3 C4 112.8(3) . . ?
N2 C3 H3A 109 . . ?
C4 C3 H3A 109 . . ?
N2 C3 H3B 109 . . ?
C4 C3 H3B 109 . . ?
H3A C3 H3B 107.8 . . ?
N3 C4 C3 111.4(3) . . ?
N3 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
N3 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108 . . ?
N3 C5 C6 111.0(3) . . ?
N3 C5 H5A 109.4 . . ?
C6 C5 H5A 109.4 . . ?
N3 C5 H5B 109.4 . . ?
C6 C5 H5B 109.4 . . ?
H5A C5 H5B 108 . . ?
N1 C6 C5 107.4(3) . . ?
N1 C6 H6A 110.2 . . ?
C5 C6 H6A 110.2 . . ?
N1 C6 H6B 110.2 . . ?
C5 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
N1 C7 C8 112.5(2) . . ?
N1 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
N1 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
N4 C8 C7 124.8(3) . . ?
N4 C8 S1 114.5(2) . . ?
C7 C8 S1 120.6(2) . . ?
C10 C9 S1 111.0(3) . . ?
C10 C9 H9 124.5 . . ?
S1 C9 H9 124.5 . . ?
C9 C10 N4 114.0(3) . . ?
C9 C10 C11 126.0(3) . . ?
N4 C10 C11 119.8(3) . . ?
O2 C11 O1 127.6(3) . . ?
O2 C11 C10 116.9(3) . . ?
O1 C11 C10 115.5(3) . . ?
N2 C12 C13 111.1(3) . . ?
N2 C12 H12A 109.4 . . ?
C13 C12 H12A 109.4 . . ?
N2 C12 H12B 109.4 . . ?
C13 C12 H12B 109.4 . . ?
H12A C12 H12B 108 . . ?
N5 C13 C12 125.3(3) . . ?
N5 C13 S2 113.4(2) . . ?
C12 C13 S2 121.3(2) . . ?
C15 C14 S2 110.3(3) . . ?
C15 C14 H14 124.9 . . ?
S2 C14 H14 124.9 . . ?
C14 C15 N5 114.7(3) . . ?
C14 C15 C16 128.0(3) . . ?
N5 C15 C16 117.1(2) . . ?
O4 C16 O3 126.1(3) . . ?
O4 C16 C15 119.2(3) . . ?
O3 C16 C15 114.6(3) . . ?
N3 C17 C18 111.6(3) . . ?
N3 C17 H17A 109.3 . . ?
C18 C17 H17A 109.3 . . ?
N3 C17 H17B 109.3 . . ?
C18 C17 H17B 109.3 . . ?
H17A C17 H17B 108 . . ?
N6 C18 C17 123.8(3) . . ?
N6 C18 S3 114.3(2) . . ?
C17 C18 S3 121.8(2) . . ?
C20 C19 S3 110.2(3) . . ?
C20 C19 H19 124.9 . . ?
S3 C19 H19 124.9 . . ?
C19 C20 N6 115.0(3) . . ?
C19 C20 C21 126.3(3) . . ?
N6 C20 C21 118.7(3) . . ?
O6 C21 O5 123.5(3) . . ?
O6 C21 C20 118.8(3) . . ?
O5 C21 C20 117.6(3) . . ?
C7 N1 C6 112.1(2) . . ?
C7 N1 C1 114.2(2) . . ?
C6 N1 C1 113.1(2) . . ?
C7 N1 H1N 107.7(15) . . ?
C6 N1 H1N 105.2(15) . . ?
C1 N1 H1N 103.6(15) . . ?
C12 N2 C2 114.1(3) . . ?
C12 N2 C3 113.8(3) . . ?
C2 N2 C3 112.8(3) . . ?
C5 N3 C17 113.8(3) . . ?
C5 N3 C4 115.2(3) . . ?
C17 N3 C4 112.9(3) . . ?
C8 N4 C10 110.9(2) . . ?
C8 N4 Cu 133.9(2) . . ?
C10 N4 Cu 113.88(19) . . ?
C13 N5 C15 111.2(2) . . ?
C13 N5 Cu 139.6(2) . . ?
C15 N5 Cu 108.96(18) . . ?
C18 N6 C20 110.6(3) . . ?
C18 N6 Cu 144.1(2) . . ?
C20 N6 Cu 103.10(18) . . ?
C11 O1 Cu 113.7(2) . . ?
C16 O3 Cu 117.16(19) . . ?
C21 O5 Cu 122.3(2) . . ?
C9 S1 C8 89.58(15) . . ?
C14 S2 C13 90.46(15) . . ?
C19 S3 C18 89.86(17) . . ?
O5 Cu O3 89.36(9) . . ?
O5 Cu N5 170.40(9) . . ?
O3 Cu N5 82.16(9) . . ?
O5 Cu N4 86.15(9) . . ?
O3 Cu N4 167.83(9) . . ?
N5 Cu N4 103.04(9) . . ?
O5 Cu O1 99.08(9) . . ?
O3 Cu O1 92.92(8) . . ?
N5 Cu O1 85.88(9) . . ?
N4 Cu O1 76.67(9) . . ?
O5 Cu N6 76.33(9) . . ?
O3 Cu N6 83.89(9) . . ?
N5 Cu N6 98.21(9) . . ?
N4 Cu N6 105.95(9) . . ?
O1 Cu N6 174.39(8) . . ?
H7V O7 H7W 108(4) . . ?
H8V O8 H8W 102(4) . . ?
H9V O9 H9W 100(4) . . ?
H10V O10 H10W 99(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N N2 0.885(18) 2.07(2) 2.677(4) 124.9(19) .
N1 H1N N3 0.885(18) 2.14(2) 2.710(4) 121.2(19) .
O7 H7V O2 0.844(19) 2.07(4) 2.821(4) 147(5) 1_456
O7 H7W O2 0.843(19) 2.06(2) 2.894(4) 170(5) 2_656
O8 H8V O7 0.865(19) 1.94(2) 2.785(5) 167(5) .
O8 H8W O4 0.837(19) 2.06(2) 2.877(4) 164(5) 2_666
O9 H9V O8 0.888(19) 2.05(3) 2.887(5) 156(5) .
O9 H9W O6 0.889(19) 1.98(3) 2.792(4) 151(5) 1_455
O10 H10V O8 0.88(2) 2.04(3) 2.861(5) 155(7) .
O10 H10W O5 0.86(2) 2.21(3) 3.025(4) 158(6) 2_656

#----------------------------------------------------------------------------#
#                   SHELXL.RES FILE                                          #
#----------------------------------------------------------------------------#

_iucr_refine_instruction_details 
;
TITL Cuno3tha-f at 296 K in P-1
CELL  0.71073   8.9546  10.9939  14.0477   85.134   86.799   81.534
ZERR     2.00   0.0004   0.0005   0.0006    0.004    0.003    0.004
LATT   1
SFAC  C    H    N    O    S    CU
UNIT  42   60   12   20   6    2
MERG   2
OMIT    -1   1   1
SHEL  13 0.8
DFIX  0.91 N1 H1N
SADI  0.04 C1 H1N C6 H1N C7 H1N
DFIX  0.85 O7 H7V O7 H7W O8 H8V O8 H8W O9 H9V O9 H9W O10 H10V O10 H10W
DANG  1.34 H7V H7W H8V H8W H9V H9W H10V H10W
EQIV   $1   x-1,  y,   z+1
EQIV   $2  -x+1, -y,   -z+1
EQIV   $3  -x+1, -y+1, -z+1
EQIV   $4   x-1,  y,    z
HTAB   N1  N2
HTAB   N1  N3
HTAB   O7  O2_$1
HTAB   O7  O2_$2
HTAB   O8  O7
HTAB   O8  O4_$3
HTAB   O9  O8
HTAB   O9  O6_$4
HTAB   O10 O8
HTAB   O10 O5_$2
FMAP   2
PLAN   25
SIZE     0.05   0.08   0.27
ACTA
HTAB    2.00000
BOND   $H
L.S.  10
TEMP    23.00
WGHT    0.054700    0.138100
FVAR       1.01231
MOLE    1
C1    1    0.079429    0.084933    0.264556    11.00000    0.03509    0.03443 =
         0.05386   -0.00801   -0.00264   -0.01382
AFIX  23
H1A   2   -0.025937    0.110690    0.282513    11.00000   -1.20000
H1B   2    0.098812   -0.004428    0.272319    11.00000   -1.20000
AFIX   0
C2    1    0.110438    0.128324    0.160585    11.00000    0.04271    0.03124 =
         0.04749   -0.00633   -0.01101   -0.01497
AFIX  23
H2A   2    0.196101    0.075353    0.133952    11.00000   -1.20000
H2B   2    0.023205    0.123977    0.123728    11.00000   -1.20000
AFIX   0
C3    1    0.005723    0.346418    0.167864    11.00000    0.03459    0.04181 =
         0.05440   -0.00366   -0.01444   -0.00116
AFIX  23
H3A   2   -0.077248    0.303151    0.191877    11.00000   -1.20000
H3B   2   -0.020830    0.388139    0.106194    11.00000   -1.20000
AFIX   0
C4    1    0.026016    0.443322    0.237380    11.00000    0.03364    0.03393 =
         0.05136   -0.00363   -0.00309    0.00335
AFIX  23
H4A   2    0.087523    0.501781    0.205887    11.00000   -1.20000
H4B   2   -0.071949    0.488348    0.254455    11.00000   -1.20000
AFIX   0
C5    1    0.006036    0.311949    0.387054    11.00000    0.03757    0.03857 =
         0.04586   -0.00859    0.01062   -0.00657
AFIX  23
H5A   2   -0.082967    0.300369    0.354506    11.00000   -1.20000
H5B   2   -0.027195    0.355145    0.443594    11.00000   -1.20000
AFIX   0
C6    1    0.095117    0.186227    0.416796    11.00000    0.04317    0.03889 =
         0.03837   -0.00142    0.01293   -0.00593
AFIX  23
H6A   2    0.165834    0.194476    0.464897    11.00000   -1.20000
H6B   2    0.026986    0.129935    0.443346    11.00000   -1.20000
AFIX   0
C7    1    0.321582    0.055783    0.351885    11.00000    0.03831    0.02884 =
         0.03464    0.00276    0.00209   -0.00824
AFIX  23
H7A   2    0.297437   -0.021445    0.383170    11.00000   -1.20000
H7B   2    0.375727    0.094206    0.396263    11.00000   -1.20000
AFIX   0
C8    1    0.421728    0.029568    0.264751    11.00000    0.03043    0.02280 =
         0.03659    0.00234   -0.00325   -0.00457
C9    1    0.572795   -0.064859    0.137404    11.00000    0.04311    0.03479 =
         0.04790   -0.01449    0.00650   -0.00931
AFIX  43
H9    2    0.624490   -0.114179    0.092108    11.00000   -1.20000
AFIX   0
C10   1    0.586475    0.055362    0.143788    11.00000    0.02940    0.02988 =
         0.03558   -0.00518    0.00113   -0.00672
C11   1    0.694337    0.127290    0.084393    11.00000    0.03168    0.03609 =
         0.03426    0.00121   -0.00340   -0.00554
C12   1    0.240295    0.288016    0.073616    11.00000    0.03814    0.03967 =
         0.03448   -0.00369   -0.00949   -0.00573
AFIX  23
H12A  2    0.181470    0.305042    0.016852    11.00000   -1.20000
H12B  2    0.318338    0.218781    0.063016    11.00000   -1.20000
AFIX   0
C13   1    0.312047    0.398336    0.089678    11.00000    0.03409    0.03506 =
         0.02890    0.00105   -0.00524   -0.00580
C14   1    0.383539    0.602593    0.087094    11.00000    0.04665    0.03367 =
         0.04365    0.00719   -0.00785   -0.00860
AFIX  43
H14   2    0.397528    0.685045    0.078732    11.00000   -1.20000
AFIX   0
C15   1    0.458573    0.517100    0.149015    11.00000    0.03367    0.02663 =
         0.03031   -0.00042    0.00167   -0.00677
C16   1    0.587920    0.531000    0.208823    11.00000    0.03311    0.03359 =
         0.03337   -0.00424    0.00088   -0.00795
C17   1    0.171145    0.471031    0.373505    11.00000    0.04087    0.03366 =
         0.04840   -0.01342    0.00272   -0.00289
AFIX  23
H17A  2    0.097640    0.515092    0.416317    11.00000   -1.20000
H17B  2    0.208203    0.531102    0.326956    11.00000   -1.20000
AFIX   0
C18   1    0.300207    0.404695    0.429735    11.00000    0.04553    0.03708 =
         0.03393   -0.00811   -0.00062   -0.01528
C19   1    0.482039    0.329415    0.549397    11.00000    0.05551    0.06177 =
         0.03035   -0.00256   -0.00497   -0.02317
AFIX  43
H19   2    0.540309    0.307456    0.602597    11.00000   -1.20000
AFIX   0
C20   1    0.520249    0.292162    0.460346    11.00000    0.04064    0.04257 =
         0.02903    0.00396   -0.00611   -0.01966
C21   1    0.661920    0.212420    0.430994    11.00000    0.03878    0.03483 =
         0.03999    0.00887   -0.00736   -0.01722
N1    3    0.178650    0.138037    0.328825    11.00000    0.03063    0.02673 =
         0.03470   -0.00055    0.00440   -0.01008
N2    3    0.142727    0.255935    0.155149    11.00000    0.03367    0.02992 =
         0.03571   -0.00380   -0.00728   -0.00504
N3    3    0.097904    0.385803    0.324127    11.00000    0.03172    0.02956 =
         0.04246   -0.00589   -0.00155   -0.00675
N4    3    0.499209    0.109194    0.216853    11.00000    0.02875    0.02448 =
         0.02838    0.00044   -0.00163   -0.00194
N5    3    0.415988    0.401064    0.151188    11.00000    0.02918    0.02522 =
         0.02714    0.00032   -0.00127   -0.00710
N6    3    0.415108    0.334158    0.392494    11.00000    0.03571    0.03305 =
         0.02953   -0.00404   -0.00090   -0.00797
O1    4    0.701110    0.232721    0.109259    11.00000    0.03862    0.03436 =
         0.04466   -0.00042    0.00425   -0.00954
O2    4    0.765841    0.075459    0.016529    11.00000    0.05903    0.05331 =
         0.05105   -0.01811    0.02503   -0.01655
O3    4    0.642660    0.432770    0.257055    11.00000    0.03563    0.03528 =
         0.03766   -0.00117   -0.01042   -0.00658
O4    4    0.632813    0.632235    0.206711    11.00000    0.05318    0.03060 =
         0.07658   -0.00530   -0.01455   -0.01549
O5    4    0.682923    0.192759    0.342816    11.00000    0.03730    0.03471 =
         0.03855    0.00146   -0.00962   -0.00294
O6    4    0.752656    0.168584    0.493044    11.00000    0.04542    0.07535 =
         0.04614    0.02276   -0.01845   -0.01604
S1    5    0.448798   -0.113388    0.223055    11.00000    0.04775    0.02623 =
         0.05906   -0.00715    0.01005   -0.01100
S2    5    0.260586    0.537893    0.027063    11.00000    0.04749    0.04104 =
         0.04203    0.01124   -0.01643   -0.00678
S3    5    0.312221    0.422007    0.549437    11.00000    0.06636    0.06286 =
         0.03469   -0.01538    0.00608   -0.01871
CU    6    0.550708    0.281984    0.243391    11.00000    0.03176    0.02545 =
         0.03059    0.00074   -0.00686   -0.00615
H1N   2    0.202964    0.204109    0.294462    11.00000   -1.20000
MOLE    2
O7    4    0.030730    0.142868    0.921347    11.00000    0.06483    0.07137 =
         0.07616    0.01172    0.00832   -0.01837
H7V   2   -0.062111    0.136380    0.928385    11.00000   -1.50000
H7W   2    0.080469    0.074278    0.939163    11.00000   -1.50000
MOLE    3
O8    4    0.125161    0.243075    0.743320    11.00000    0.07333    0.06557 =
         0.06878    0.00254   -0.01157   -0.02676
H8V   2    0.089755    0.223993    0.800285    11.00000   -1.50000
H8W   2    0.184109    0.292414    0.753794    11.00000   -1.50000
MOLE    4
O9    4   -0.166298    0.228146    0.670620    11.00000    0.09325    0.08042 =
         0.08503   -0.00013   -0.01524   -0.02954
H9V   2   -0.072687    0.243697    0.675956    11.00000   -1.50000
H9W   2   -0.167872    0.225930    0.607605    11.00000   -1.50000
MOLE    5
O10   4    0.279359    0.082944    0.607841    11.00000    0.16596    0.06421 =
         0.08404    0.00268   -0.02724   -0.00214
H10V  2    0.208830    0.120129    0.645784    11.00000   -1.50000
H10W  2    0.263225    0.007823    0.620862    11.00000   -1.50000
HKLF    4
 
REM  Cuno3tha-f at 296 K in P-1
REM R1 =  0.0468 for   4356 Fo > 4sig(Fo)  and  0.0630 for all   5560 data
REM    397 parameters refined using     16 restraints
 
END
 
WGHT      0.0549      0.1263
REM Highest difference peak  0.403,  deepest hole -0.508,  1-sigma level  0.080
Q1    1   0.4526  0.2491  0.2507  11.00000  0.05    0.40
Q2    1   0.3864  0.3623  0.5593  11.00000  0.05    0.37
Q3    1   0.2471  0.4446  0.4007  11.00000  0.05    0.37
Q4    1   0.5021  0.3926  0.2604  11.00000  0.05    0.35
Q5    1   0.6097  0.4355  0.2759  11.00000  0.05    0.35
Q6    1   0.2925  0.5959  0.0773  11.00000  0.05    0.35
Q7    1   0.5147  0.2146  0.1801  11.00000  0.05    0.34
Q8    1   0.0767  0.5638  0.4014  11.00000  0.05    0.34
Q9    1   0.4559  0.3451  0.2103  11.00000  0.05    0.34
Q10   1   0.5768  0.3548  0.3067  11.00000  0.05    0.33
Q11   1   0.1730  0.0626  0.5963  11.00000  0.05    0.33
Q12   1   0.4532 -0.0561  0.2636  11.00000  0.05    0.30
Q13   1   0.3838  0.3845  0.1444  11.00000  0.05    0.30
Q14   1   0.1124  0.4164  0.3429  11.00000  0.05    0.30
Q15   1   0.4706  0.4533  0.1497  11.00000  0.05    0.30
Q16   1   0.3680 -0.0545  0.2023  11.00000  0.05    0.29
Q17   1   0.6825  0.2990  0.2375  11.00000  0.05    0.29
Q18   1   0.6581  0.2196  0.2755  11.00000  0.05    0.29
Q19   1  -0.0357  0.3122  0.4011  11.00000  0.05    0.29
Q20   1   0.5234  0.5202  0.1823  11.00000  0.05    0.29
Q21   1   0.4749  0.3195  0.0950  11.00000  0.05    0.28
Q22   1   0.3372 -0.1417  0.2372  11.00000  0.05    0.28
Q23   1   0.3448  0.4048  0.1786  11.00000  0.05    0.27
Q24   1   0.0389  0.3889  0.1939  11.00000  0.05    0.27
Q25   1   0.7278  0.1951  0.1351  11.00000  0.05    0.27
;

#----------------------------------------------------------------------------#
#                   END OF CIF                                               #
#----------------------------------------------------------------------------#

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cuno2th1tha-e_296k
_database_code_depnum_ccdc_archive 'CCDC 1903039'
loop_
_audit_author_name
_audit_author_address
'francois michaud'
;UNIVERSITE DE BRETAGNE OCCIDENTALE
France
;
_audit_update_record             
;
2019-03-13 deposited with the CCDC.	2019-05-17 downloaded from the CCDC.
;

_audit_creation_date             2017-09-18T15:53:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
;
        C38 H46 Cu3 N12 O4 S6 4+, (Cl O4 1-)4, 2(H2 O)
;
_chemical_formula_sum            'C38 H50 Cl4 Cu3 N12 O22 S6'
_chemical_formula_weight         1551.68

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  -P1
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7341(6)
_cell_length_b                   10.4174(7)
_cell_length_c                   14.3026(8)
_cell_angle_alpha                87.718(5)
_cell_angle_beta                 89.646(5)
_cell_angle_gamma                80.050(5)
_cell_volume                     1427.39(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6663
_cell_measurement_theta_min      4.06
_cell_measurement_theta_max      26.428

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       'fragment of flat rounded needle'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             789
_exptl_crystal_recrystallization_method 
'from aqueous solution at room temperature,by slow evaporation of water'
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.6545
_exptl_absorpt_correction_T_max  0.9242

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_orient_matrix_ub_11      -0.0318121
_diffrn_orient_matrix_ub_12      0.022859
_diffrn_orient_matrix_ub_13      -0.0434092
_diffrn_orient_matrix_ub_21      0.0611699
_diffrn_orient_matrix_ub_22      -0.0283669
_diffrn_orient_matrix_ub_23      -0.0238778
_diffrn_orient_matrix_ub_31      -0.0268468
_diffrn_orient_matrix_ub_32      -0.0588172
_diffrn_orient_matrix_ub_33      -0.0030502
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0962
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_number            17173
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.41
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             5817
_reflns_number_gt                4621
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
;
        ORTEP3 for Windows (Farrugia, 1997)
        MERCURY  (Bruno et al., 2002)
;
_computing_publication_material  
;
        WinGX (Farrugia, 1999)
        PLATON (Spek, 1990-2003)
        enCIFer (Allen et al., 2004)
;

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0610P)²+1.6337P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5817
_refine_ls_number_parameters     406
_refine_ls_number_restraints     168
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.153
_refine_ls_wR_factor_gt          0.1406
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.124
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.098

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4797(5) 0.3583(5) 0.2289(3) 0.0420(11) Uani 1 1 d . . .
H1A H 0.5458 0.3349 0.1788 0.05 Uiso 1 1 calc R . .
H1B H 0.5289 0.3898 0.2796 0.05 Uiso 1 1 calc R . .
C2 C 0.3650(5) 0.4647(4) 0.1941(3) 0.0422(11) Uani 1 1 d . . .
H2A H 0.3115 0.5016 0.247 0.051 Uiso 1 1 calc R . .
H2B H 0.4058 0.5335 0.1628 0.051 Uiso 1 1 calc R . .
C3 C 0.3376(6) 0.3767(5) 0.0365(3) 0.0443(11) Uani 1 1 d . . .
H3A H 0.4378 0.37 0.0422 0.053 Uiso 1 1 calc R . .
H3B H 0.3053 0.4431 -0.0117 0.053 Uiso 1 1 calc R . .
C4 C 0.3035(6) 0.2467(5) 0.0083(3) 0.0446(11) Uani 1 1 d . . .
H4A H 0.2083 0.2588 -0.0144 0.054 Uiso 1 1 calc R . .
H4B H 0.365 0.2127 -0.0418 0.054 Uiso 1 1 calc R . .
C5 C 0.4711(5) 0.1124(5) 0.1184(3) 0.0440(11) Uani 1 1 d . . .
H5A H 0.5253 0.17 0.0857 0.053 Uiso 1 1 calc R . .
H5B H 0.5045 0.0245 0.0985 0.053 Uiso 1 1 calc R . .
C6 C 0.4961(5) 0.1167(5) 0.2228(3) 0.0412(11) Uani 1 1 d . . .
H6A H 0.4641 0.0433 0.2544 0.049 Uiso 1 1 calc R . .
H6B H 0.5954 0.1084 0.2342 0.049 Uiso 1 1 calc R . .
C7 C 0.4089(5) 0.2293(4) 0.3658(3) 0.0363(10) Uani 1 1 d . . .
H7A H 0.3694 0.152 0.3821 0.044 Uiso 1 1 calc R . .
H7B H 0.344 0.3042 0.3864 0.044 Uiso 1 1 calc R . .
C8 C 0.5452(5) 0.2214(4) 0.4179(3) 0.0378(10) Uani 1 1 d . . .
C9 C 0.7791(5) 0.1632(5) 0.4826(3) 0.0445(11) Uani 1 1 d . . .
H9 H 0.8685 0.1266 0.5026 0.053 Uiso 1 1 calc R . .
C10 C 0.7174(5) 0.2879(4) 0.4957(3) 0.0358(10) Uani 1 1 d . . .
C11 C 0.7699(5) 0.3924(5) 0.5459(3) 0.0434(11) Uani 1 1 d . . .
C12 C 0.1375(5) 0.5105(5) 0.1145(3) 0.0433(11) Uani 1 1 d . . .
H12A H 0.157 0.5987 0.1082 0.052 Uiso 1 1 calc R . .
H12B H 0.0904 0.4923 0.0582 0.052 Uiso 1 1 calc R . .
C13 C 0.0482(5) 0.4972(4) 0.1976(3) 0.0391(10) Uani 1 1 d . . .
C14 C -0.1263(6) 0.5053(5) 0.3188(4) 0.0519(13) Uani 1 1 d . . .
H14 H -0.1998 0.5231 0.3608 0.062 Uiso 1 1 calc R . .
C15 C -0.0314(5) 0.3949(5) 0.3203(4) 0.0459(12) Uani 1 1 d . . .
H15 H -0.0323 0.3276 0.3649 0.055 Uiso 1 1 calc R . .
C16 C 0.2503(6) 0.0380(5) 0.0764(3) 0.0453(12) Uani 1 1 d . . .
H16A H 0.3182 -0.0365 0.0585 0.054 Uiso 1 1 calc R . .
H16B H 0.1819 0.0589 0.0266 0.054 Uiso 1 1 calc R . .
C17 C 0.1798(5) 0.0054(4) 0.1654(3) 0.0405(11) Uani 1 1 d . . .
C18 C 0.0522(7) -0.0728(6) 0.2941(4) 0.0611(16) Uani 1 1 d . . .
H18 H 0.0028 -0.1164 0.3371 0.073 Uiso 1 1 calc R . .
C19 C 0.0841(6) 0.0442(5) 0.3057(3) 0.0494(13) Uani 1 1 d . . .
H19 H 0.0606 0.0912 0.3591 0.059 Uiso 1 1 calc R . .
N1 N 0.4225(4) 0.2403(3) 0.2627(2) 0.0325(8) Uani 1 1 d . . .
N2 N 0.2696(4) 0.4160(3) 0.1278(3) 0.0351(8) Uani 1 1 d . . .
N3 N 0.3209(4) 0.1515(4) 0.0906(2) 0.0367(8) Uani 1 1 d . . .
N4 N 0.5845(4) 0.3209(3) 0.4580(2) 0.0341(8) Uani 1 1 d . . .
N5 N 0.0674(4) 0.3896(4) 0.2502(3) 0.0363(8) Uani 1 1 d . . .
N6 N 0.1558(4) 0.0903(4) 0.2309(3) 0.0360(8) Uani 1 1 d . . .
O1 O 0.6845(3) 0.4996(3) 0.5483(3) 0.0478(9) Uani 1 1 d . . .
O2 O 0.8868(4) 0.3706(4) 0.5809(3) 0.0642(11) Uani 1 1 d . . .
S1 S 0.66995(15) 0.08294(13) 0.42447(10) 0.0519(3) Uani 1 1 d . . .
S2 S -0.09281(14) 0.60829(12) 0.22905(10) 0.0478(3) Uani 1 1 d . . .
S3 S 0.1141(2) -0.13285(14) 0.18956(11) 0.0659(5) Uani 1 1 d . . .
Cu1 Cu 0.21467(5) 0.25729(5) 0.19589(3) 0.03080(17) Uani 1 1 d . . .
Cu2 Cu 0.5 0.5 0.5 0.0383(2) Uani 1 2 d S . .
O3A O 0.7935(10) 0.3719(8) 0.1203(6) 0.078(3) Uiso 0.5 1 d PD A 1
O4A O 0.9688(9) 0.2386(11) 0.0353(7) 0.074(3) Uiso 0.5 1 d PD A 1
O5A O 0.8192(11) 0.1361(10) 0.1337(8) 0.084(3) Uiso 0.5 1 d PD A 1
O6A O 0.7384(9) 0.2477(8) -0.0014(6) 0.051(2) Uiso 0.5 1 d PD A 1
Cl1A Cl 0.8284(4) 0.2547(4) 0.0790(4) 0.0441(13) Uiso 0.5 1 d PD A 1
O3B O 0.8768(17) 0.0910(11) 0.0825(12) 0.077(4) Uiso 0.3 1 d PD B 2
O4B O 0.8098(16) 0.2660(17) 0.1778(9) 0.080(4) Uiso 0.3 1 d PD B 2
O5B O 0.9695(10) 0.2840(13) 0.0576(8) 0.033(2) Uiso 0.3 1 d PD B 2
O6B O 0.729(2) 0.285(2) 0.0287(18) 0.099(11) Uiso 0.3 1 d PD B 2
Cl1B Cl 0.8498(7) 0.2284(8) 0.0854(5) 0.041(2) Uiso 0.3 1 d PD B 2
O3C O 0.8247(16) 0.1870(17) 0.1667(9) 0.035(3) Uiso 0.2 1 d PD C 3
O4C O 0.917(3) 0.338(2) 0.0809(16) 0.080(7) Uiso 0.2 1 d PD C 3
O5C O 0.924(3) 0.133(2) 0.0194(18) 0.112(10) Uiso 0.2 1 d PD C 3
O6C O 0.7103(19) 0.278(3) 0.0221(18) 0.040(6) Uiso 0.2 1 d PD C 3
Cl1C Cl 0.8394(11) 0.2332(12) 0.0678(7) 0.035(3) Uiso 0.2 1 d PD C 3
O7 O 0.5301(5) 0.6272(4) 0.3348(3) 0.0741(12) Uani 1 1 d D . .
O8 O 0.4303(6) 0.8491(5) 0.3436(4) 0.104(2) Uani 1 1 d D . .
O9 O 0.6666(6) 0.7878(6) 0.3310(6) 0.135(3) Uani 1 1 d D . .
O10 O 0.5300(8) 0.7696(6) 0.2067(4) 0.125(2) Uani 1 1 d D . .
Cl2 Cl 0.53745(14) 0.75826(13) 0.30458(10) 0.0522(3) Uani 1 1 d D . .
O11 O 0.1191(5) 0.1960(5) 0.5198(3) 0.0696(12) Uani 1 1 d D . .
H11V H 0.200(3) 0.206(7) 0.537(5) 0.104 Uiso 1 1 d D . .
H11W H 0.065(6) 0.252(6) 0.551(5) 0.104 Uiso 1 1 d D . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.497(5) . ?
C1 C2 1.502(7) . ?
C1 H1A 0.97 . ?
C1 H1B 0.97 . ?
C2 N2 1.494(6) . ?
C2 H2A 0.97 . ?
C2 H2B 0.97 . ?
C3 N2 1.499(6) . ?
C3 C4 1.519(7) . ?
C3 H3A 0.97 . ?
C3 H3B 0.97 . ?
C4 N3 1.500(6) . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
C5 N3 1.500(6) . ?
C5 C6 1.517(7) . ?
C5 H5A 0.97 . ?
C5 H5B 0.97 . ?
C6 N1 1.494(6) . ?
C6 H6A 0.97 . ?
C6 H6B 0.97 . ?
C7 N1 1.481(6) . ?
C7 C8 1.515(6) . ?
C7 H7A 0.97 . ?
C7 H7B 0.97 . ?
C8 N4 1.319(6) . ?
C8 S1 1.717(5) . ?
C9 C10 1.353(6) . ?
C9 S1 1.701(5) . ?
C9 H9 0.93 . ?
C10 N4 1.386(6) . ?
C10 C11 1.490(6) . ?
C11 O2 1.227(6) . ?
C11 O1 1.273(6) . ?
C12 C13 1.485(7) . ?
C12 N2 1.487(6) . ?
C12 H12A 0.97 . ?
C12 H12B 0.97 . ?
C13 N5 1.312(6) . ?
C13 S2 1.706(5) . ?
C14 C15 1.344(7) . ?
C14 S2 1.706(6) . ?
C14 H14 0.93 . ?
C15 N5 1.382(6) . ?
C15 H15 0.93 . ?
C16 N3 1.488(6) . ?
C16 C17 1.497(7) . ?
C16 H16A 0.97 . ?
C16 H16B 0.97 . ?
C17 N6 1.307(6) . ?
C17 S3 1.697(5) . ?
C18 C19 1.325(7) . ?
C18 S3 1.710(6) . ?
C18 H18 0.93 . ?
C19 N6 1.388(6) . ?
C19 H19 0.93 . ?
N1 Cu1 2.219(4) . ?
N2 Cu1 2.034(4) . ?
N3 Cu1 2.066(4) . ?
N4 Cu2 2.017(4) . ?
N5 Cu1 1.986(4) . ?
N6 Cu1 1.969(4) . ?
O1 Cu2 1.927(3) . ?
Cu2 O1 1.927(3) 2_666 ?
Cu2 N4 2.017(4) 2_666 ?
O3A Cl1A 1.366(8) . ?
O4A Cl1A 1.485(9) . ?
O5A Cl1A 1.452(9) . ?
O6A Cl1A 1.461(8) . ?
O3B Cl1B 1.412(12) . ?
O4B Cl1B 1.427(12) . ?
O5B Cl1B 1.436(9) . ?
O6B Cl1B 1.455(13) . ?
O3C Cl1C 1.489(12) . ?
O4C Cl1C 1.454(13) . ?
O5C Cl1C 1.411(14) . ?
O6C Cl1C 1.417(13) . ?
O7 Cl2 1.429(4) . ?
O8 Cl2 1.411(4) . ?
O9 Cl2 1.402(5) . ?
O10 Cl2 1.401(5) . ?
O11 H11V 0.85(2) . ?
O11 H11W 0.85(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 111.1(4) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108 . . ?
N2 C2 C1 112.1(4) . . ?
N2 C2 H2A 109.2 . . ?
C1 C2 H2A 109.2 . . ?
N2 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N2 C3 C4 110.7(4) . . ?
N2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
N3 C4 C3 110.0(4) . . ?
N3 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
N3 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N3 C5 C6 113.7(4) . . ?
N3 C5 H5A 108.8 . . ?
C6 C5 H5A 108.8 . . ?
N3 C5 H5B 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
N1 C6 C5 112.2(4) . . ?
N1 C6 H6A 109.2 . . ?
C5 C6 H6A 109.2 . . ?
N1 C6 H6B 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
N1 C7 C8 113.9(4) . . ?
N1 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
N1 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
N4 C8 C7 124.0(4) . . ?
N4 C8 S1 112.9(3) . . ?
C7 C8 S1 123.0(3) . . ?
C10 C9 S1 110.4(3) . . ?
C10 C9 H9 124.8 . . ?
S1 C9 H9 124.8 . . ?
C9 C10 N4 114.3(4) . . ?
C9 C10 C11 129.6(4) . . ?
N4 C10 C11 116.0(4) . . ?
O2 C11 O1 125.7(4) . . ?
O2 C11 C10 119.8(4) . . ?
O1 C11 C10 114.5(4) . . ?
C13 C12 N2 107.9(4) . . ?
C13 C12 H12A 110.1 . . ?
N2 C12 H12A 110.1 . . ?
C13 C12 H12B 110.1 . . ?
N2 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
N5 C13 C12 120.6(4) . . ?
N5 C13 S2 113.8(4) . . ?
C12 C13 S2 125.4(3) . . ?
C15 C14 S2 110.5(4) . . ?
C15 C14 H14 124.8 . . ?
S2 C14 H14 124.8 . . ?
C14 C15 N5 114.5(5) . . ?
C14 C15 H15 122.7 . . ?
N5 C15 H15 122.7 . . ?
N3 C16 C17 109.2(4) . . ?
N3 C16 H16A 109.8 . . ?
C17 C16 H16A 109.8 . . ?
N3 C16 H16B 109.8 . . ?
C17 C16 H16B 109.8 . . ?
H16A C16 H16B 108.3 . . ?
N6 C17 C16 120.3(4) . . ?
N6 C17 S3 113.6(4) . . ?
C16 C17 S3 126.0(3) . . ?
C19 C18 S3 110.9(4) . . ?
C19 C18 H18 124.6 . . ?
S3 C18 H18 124.6 . . ?
C18 C19 N6 114.0(5) . . ?
C18 C19 H19 123 . . ?
N6 C19 H19 123 . . ?
C7 N1 C6 112.3(3) . . ?
C7 N1 C1 113.6(3) . . ?
C6 N1 C1 113.4(4) . . ?
C7 N1 Cu1 110.0(3) . . ?
C6 N1 Cu1 100.6(3) . . ?
C1 N1 Cu1 105.8(3) . . ?
C12 N2 C2 111.2(4) . . ?
C12 N2 C3 112.1(4) . . ?
C2 N2 C3 113.2(4) . . ?
C12 N2 Cu1 105.5(3) . . ?
C2 N2 Cu1 104.6(3) . . ?
C3 N2 Cu1 109.6(3) . . ?
C16 N3 C4 112.3(4) . . ?
C16 N3 C5 113.0(4) . . ?
C4 N3 C5 111.7(4) . . ?
C16 N3 Cu1 107.1(3) . . ?
C4 N3 Cu1 103.1(3) . . ?
C5 N3 Cu1 109.0(3) . . ?
C8 N4 C10 111.7(4) . . ?
C8 N4 Cu2 139.0(3) . . ?
C10 N4 Cu2 108.4(3) . . ?
C13 N5 C15 111.1(4) . . ?
C13 N5 Cu1 110.4(3) . . ?
C15 N5 Cu1 137.9(3) . . ?
C17 N6 C19 111.6(4) . . ?
C17 N6 Cu1 113.0(3) . . ?
C19 N6 Cu1 135.2(3) . . ?
C11 O1 Cu2 116.6(3) . . ?
C9 S1 C8 90.7(2) . . ?
C13 S2 C14 90.0(2) . . ?
C17 S3 C18 90.0(2) . . ?
N6 Cu1 N5 103.68(16) . . ?
N6 Cu1 N2 166.13(15) . . ?
N5 Cu1 N2 83.17(15) . . ?
N6 Cu1 N3 83.52(15) . . ?
N5 Cu1 N3 156.00(15) . . ?
N2 Cu1 N3 85.57(15) . . ?
N6 Cu1 N1 103.65(14) . . ?
N5 Cu1 N1 114.49(14) . . ?
N2 Cu1 N1 83.89(14) . . ?
N3 Cu1 N1 85.16(14) . . ?
O1 Cu2 O1 180 . 2_666 ?
O1 Cu2 N4 83.54(14) . . ?
O1 Cu2 N4 96.46(14) 2_666 . ?
O1 Cu2 N4 96.46(14) . 2_666 ?
O1 Cu2 N4 83.54(14) 2_666 2_666 ?
N4 Cu2 N4 180.00(19) . 2_666 ?
O3A Cl1A O5A 118.8(7) . . ?
O3A Cl1A O6A 110.8(6) . . ?
O5A Cl1A O6A 103.4(6) . . ?
O3A Cl1A O4A 112.2(7) . . ?
O5A Cl1A O4A 107.8(6) . . ?
O6A Cl1A O4A 102.2(6) . . ?
O3B Cl1B O4B 109.6(10) . . ?
O3B Cl1B O5B 111.6(10) . . ?
O4B Cl1B O5B 109.3(9) . . ?
O3B Cl1B O6B 111.7(12) . . ?
O4B Cl1B O6B 103.7(13) . . ?
O5B Cl1B O6B 110.5(12) . . ?
O5C Cl1C O6C 112.2(15) . . ?
O5C Cl1C O4C 108.9(14) . . ?
O6C Cl1C O4C 112.1(15) . . ?
O5C Cl1C O3C 108.8(14) . . ?
O6C Cl1C O3C 113.7(12) . . ?
O4C Cl1C O3C 100.5(11) . . ?
O10 Cl2 O9 107.4(5) . . ?
O10 Cl2 O8 109.8(4) . . ?
O9 Cl2 O8 108.8(4) . . ?
O10 Cl2 O7 109.5(3) . . ?
O9 Cl2 O7 109.2(4) . . ?
O8 Cl2 O7 112.1(3) . . ?
H11V O11 H11W 103(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O11 H11V O9 0.85(2) 2.31(5) 3.023(8) 142(7) 2_666
O11 H11W O2 0.85(2) 2.01(3) 2.805(6) 156(7) 1_455

#----------------------------------------------------------------------------#
#                   SHELXL.RES FILE                                          #
#----------------------------------------------------------------------------#

_iucr_refine_instruction_details 
;
TITL Cuno2th1tha-e at 296 K in P-1
CELL  0.71073   9.7341  10.4174  14.3026   87.718   89.646   80.050
ZERR     1.00   0.0006   0.0007   0.0008    0.005    0.005    0.005
LATT   1
SFAC  C    H    N    O    S    CU   CL
UNIT  38   50   12   22   6    3    4
MERG   2
SHEL  13 0.8
SADI  CL1A O3A CL1A O4A CL1A O5A CL1A O6A CL1B O3B CL1B O4B CL1B O5B CL1B O6B
SADI  CL1C O3C CL1C O4C CL1C O5C CL1C O6C
SADI  0.04 O3A O4A O3A O5A O3A O6A O4A O5A O4A O6A O5A O6A
SADI  0.04 O3B O4B O3B O5B O3B O6B O4B O5B O4B O6B O5B O6B
SADI  0.04 O3C O4C O3C O5C O3C O6C O4C O5C O4C O6C O5C O6C
SADI  CL2 O7 CL2 O8 CL2 O9 CL2 O10 CL1A O3A CL1C O3C
DFIX  0.85 O11 H11V O11 H11W
DANG  1.34 H11V H11W
EQIV  $1 -x+1, -y+1, -z+1
EQIV  $2  x-1,  y,    z
HTAB   O11 O9_$1
HTAB   O11 O2_$2
FMAP   2
PLAN   20
SIZE     0.05   0.15   0.35
ACTA
BOND   $H
L.S.   4
TEMP    23.00
WGHT    0.061000    1.633700
FVAR       1.21573
MOLE    1
 
C1    1    0.479686    0.358324    0.228906    11.00000    0.04541    0.04144 =
         0.04303   -0.00287    0.00031   -0.01837
AFIX  23
H1A   2    0.545754    0.334898    0.178792    11.00000   -1.20000
H1B   2    0.528904    0.389839    0.279613    11.00000   -1.20000
AFIX   0
C2    1    0.365046    0.464696    0.194077    11.00000    0.04608    0.03510 =
         0.04812   -0.00230    0.00168   -0.01436
AFIX  23
H2A   2    0.311538    0.501640    0.246977    11.00000   -1.20000
H2B   2    0.405838    0.533458    0.162850    11.00000   -1.20000
AFIX   0
C3    1    0.337582    0.376741    0.036472    11.00000    0.05045    0.04500 =
         0.03795    0.00289    0.01106   -0.01141
AFIX  23
H3A   2    0.437839    0.370001    0.042200    11.00000   -1.20000
H3B   2    0.305257    0.443064   -0.011710    11.00000   -1.20000
AFIX   0
C4    1    0.303518    0.246718    0.008325    11.00000    0.05244    0.05182 =
         0.03147   -0.00114    0.00652   -0.01476
AFIX  23
H4A   2    0.208266    0.258816   -0.014357    11.00000   -1.20000
H4B   2    0.365028    0.212656   -0.041848    11.00000   -1.20000
AFIX   0
C5    1    0.471122    0.112404    0.118416    11.00000    0.04466    0.04271 =
         0.04255   -0.00989    0.00628   -0.00044
AFIX  23
H5A   2    0.525296    0.169988    0.085692    11.00000   -1.20000
H5B   2    0.504515    0.024549    0.098539    11.00000   -1.20000
AFIX   0
C6    1    0.496115    0.116739    0.222751    11.00000    0.04062    0.03782 =
         0.04332   -0.00524   -0.00053   -0.00048
AFIX  23
H6A   2    0.464086    0.043257    0.254373    11.00000   -1.20000
H6B   2    0.595445    0.108438    0.234158    11.00000   -1.20000
AFIX   0
C7    1    0.408855    0.229278    0.365813    11.00000    0.03777    0.03580 =
         0.03596   -0.00524   -0.00214   -0.00729
AFIX  23
H7A   2    0.369446    0.151974    0.382142    11.00000   -1.20000
H7B   2    0.344002    0.304226    0.386444    11.00000   -1.20000
AFIX   0
C8    1    0.545240    0.221372    0.417916    11.00000    0.03900    0.03685 =
         0.03666   -0.00388   -0.00042   -0.00358
C9    1    0.779077    0.163229    0.482635    11.00000    0.03774    0.04275 =
         0.04957   -0.00388   -0.01298    0.00367
AFIX  43
H9    2    0.868528    0.126614    0.502612    11.00000   -1.20000
AFIX   0
C10   1    0.717367    0.287873    0.495736    11.00000    0.03310    0.03873 =
         0.03442   -0.00246   -0.00192   -0.00308
C11   1    0.769882    0.392394    0.545931    11.00000    0.04063    0.04551 =
         0.04473   -0.00710   -0.00801   -0.00811
C12   1    0.137527    0.510536    0.114458    11.00000    0.04883    0.03899 =
         0.04103    0.00568   -0.00044   -0.00616
AFIX  23
H12A  2    0.157009    0.598695    0.108162    11.00000   -1.20000
H12B  2    0.090393    0.492274    0.058206    11.00000   -1.20000
AFIX   0
C13   1    0.048214    0.497232    0.197632    11.00000    0.04204    0.03511 =
         0.04042    0.00062   -0.00657   -0.00744
C14   1   -0.126281    0.505330    0.318803    11.00000    0.04465    0.04909 =
         0.06083   -0.00586    0.01051   -0.00429
AFIX  43
H14   2   -0.199817    0.523091    0.360784    11.00000   -1.20000
AFIX   0
C15   1   -0.031429    0.394914    0.320322    11.00000    0.04868    0.04253 =
         0.04667   -0.00233    0.00911   -0.00832
AFIX  43
H15   2   -0.032283    0.327626    0.364934    11.00000   -1.20000
AFIX   0
C16   1    0.250260    0.037956    0.076395    11.00000    0.05609    0.04527 =
         0.04003   -0.01570    0.01063   -0.02120
AFIX  23
H16A  2    0.318230   -0.036478    0.058507    11.00000   -1.20000
H16B  2    0.181923    0.058894    0.026586    11.00000   -1.20000
AFIX   0
C17   1    0.179791    0.005392    0.165392    11.00000    0.05090    0.03306 =
         0.03994   -0.00497   -0.00163   -0.01298
C18   1    0.052184   -0.072798    0.294133    11.00000    0.08925    0.05795 =
         0.04474    0.00539    0.00974   -0.03867
AFIX  43
H18   2    0.002757   -0.116367    0.337109    11.00000   -1.20000
AFIX   0
C19   1    0.084113    0.044196    0.305692    11.00000    0.06742    0.04654 =
         0.03803    0.00076    0.01050   -0.02125
AFIX  43
H19   2    0.060607    0.091174    0.359128    11.00000   -1.20000
AFIX   0
N1    3    0.422535    0.240333    0.262722    11.00000    0.03398    0.02739 =
         0.03664   -0.00498    0.00060   -0.00551
N2    3    0.269603    0.415966    0.127750    11.00000    0.03815    0.03036 =
         0.03752   -0.00056    0.00142   -0.00858
N3    3    0.320877    0.151512    0.090638    11.00000    0.04243    0.03700 =
         0.03233   -0.00480    0.00391   -0.01054
N4    3    0.584518    0.320950    0.458023    11.00000    0.03392    0.03344 =
         0.03496   -0.00288   -0.00350   -0.00518
N5    3    0.067424    0.389556    0.250201    11.00000    0.03815    0.03514 =
         0.03533    0.00074    0.00049   -0.00577
N6    3    0.155768    0.090342    0.230922    11.00000    0.04195    0.03197 =
         0.03527   -0.00103    0.00290   -0.00962
O1    4    0.684479    0.499578    0.548285    11.00000    0.03675    0.04039 =
         0.06577   -0.01709   -0.00879   -0.00133
O2    4    0.886827    0.370623    0.580921    11.00000    0.04334    0.05845 =
         0.08962   -0.01894   -0.02708   -0.00050
S1    5    0.669950    0.082941    0.424465    11.00000    0.05439    0.03680 =
         0.06141   -0.01161   -0.01606    0.00400
S2    5   -0.092805    0.608295    0.229049    11.00000    0.04328    0.03683 =
         0.06018   -0.00107   -0.00129    0.00196
S3    5    0.114102   -0.132850    0.189563    11.00000    0.10471    0.04222 =
         0.06011   -0.00841    0.01067   -0.03753
CU1   6    0.214669    0.257293    0.195892    11.00000    0.03370    0.02827 =
         0.03126   -0.00219    0.00296   -0.00754
CU2   6    0.500000    0.500000    0.500000    10.50000    0.03145    0.03611 =
         0.04723   -0.01180   -0.00389   -0.00285
MOLE    2
PART    1
O3A   4    0.793524    0.371852    0.120266    10.50000    0.07757
O4A   4    0.968818    0.238648    0.035344    10.50000    0.07392
O5A   4    0.819185    0.136054    0.133653    10.50000    0.08419
O6A   4    0.738390    0.247670   -0.001374    10.50000    0.05096
CL1A  7    0.828372    0.254718    0.078958    10.50000    0.04415
PART    2
O3B   4    0.876832    0.091016    0.082507    10.30000    0.07682
O4B   4    0.809825    0.265969    0.177849    10.30000    0.07956
O5B   4    0.969534    0.284039    0.057570    10.30000    0.03294
O6B   4    0.729356    0.285108    0.028691    10.30000    0.09902
CL1B  7    0.849808    0.228406    0.085391    10.30000    0.04144
PART    3
O3C   4    0.824743    0.186956    0.166656    10.20000    0.03453
O4C   4    0.917396    0.338270    0.080912    10.20000    0.08034
O5C   4    0.923874    0.133500    0.019393    10.20000    0.11241
O6C   4    0.710310    0.277790    0.022071    10.20000    0.04049
CL1C  7    0.839387    0.233197    0.067818    10.20000    0.03498
MOLE    4
PART    0
O7    4    0.530117    0.627190    0.334847    11.00000    0.10077    0.04923 =
         0.07349   -0.00116    0.00907   -0.01685
O8    4    0.430253    0.849121    0.343614    11.00000    0.09523    0.06991 =
         0.12786    0.03003    0.06080    0.02947
O9    4    0.666608    0.787769    0.331019    11.00000    0.08230    0.08869 =
         0.24118   -0.04853   -0.03076   -0.02164
O10   4    0.530022    0.769645    0.206742    11.00000    0.19169    0.12051 =
         0.06005    0.01218    0.02827   -0.02156
CL2   7    0.537454    0.758259    0.304578    11.00000    0.05066    0.04486 =
         0.05896    0.00133    0.00578   -0.00349
MOLE    6
O11   4    0.119136    0.195983    0.519764    11.00000    0.05719    0.07782 =
         0.07141   -0.01360    0.00604   -0.00258
H11V  2    0.199524    0.206070    0.537111    11.00000   -1.50000
H11W  2    0.065291    0.252033    0.550656    11.00000   -1.50000
HKLF    4
 
REM  Cuno2th1tha-e at 296 K in P-1
REM R1 =  0.0558 for   4621 Fo > 4sig(Fo)  and  0.0706 for all   5817 data
REM    406 parameters refined using    168 restraints
 
END
 
WGHT      0.0610      1.6307
REM Highest difference peak  0.734,  deepest hole -0.685,  1-sigma level  0.098
Q1    1   0.7937  0.3241  0.1538  11.00000  0.05    0.73
Q2    1   0.8468  0.3779  0.0976  11.00000  0.05    0.63
Q3    1   0.9344  0.1903 -0.0019  11.00000  0.05    0.60
Q4    1   0.1650  0.3380  0.1866  11.00000  0.05    0.53
Q5    1   0.6955  0.3331  0.0588  11.00000  0.05    0.53
Q6    1   0.2726  0.1730  0.2061  11.00000  0.05    0.51
Q7    1   0.4558  0.5809  0.4815  11.00000  0.05    0.51
Q8    1   0.5891  0.8131  0.3786  11.00000  0.05    0.47
Q9    1   0.8378  0.2190  0.1988  11.00000  0.05    0.45
Q10   1   0.8916  0.1098  0.0375  11.00000  0.05    0.44
Q11   1   0.6266  0.8048  0.2404  11.00000  0.05    0.43
Q12   1   0.8172  0.1035  0.0939  11.00000  0.05    0.43
Q13   1   0.3725  0.2004  0.2038  11.00000  0.05    0.42
Q14   1   0.1326  0.3387  0.2577  11.00000  0.05    0.42
Q15   1   0.7632  0.1844  0.0201  11.00000  0.05    0.41
Q16   1   0.3940  0.8030  0.2830  11.00000  0.05    0.39
Q17   1   0.6475  0.4427  0.4960  11.00000  0.05    0.39
Q18   1   0.7420  0.3372  0.5147  11.00000  0.05    0.38
Q19   1   0.2889  0.1842  0.1290  11.00000  0.05    0.37
Q20   1   1.0001  0.2210  0.0769  11.00000  0.05    0.36
;

#----------------------------------------------------------------------------#
#                   END OF CIF                                               #
#----------------------------------------------------------------------------#

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cu-tha3-a_297k
_database_code_depnum_ccdc_archive 'CCDC 1901781'
loop_
_audit_author_name
_audit_author_address
MICHAUD
;UNIVERSITE DE BRETAGNE OCCIDENTALE
France
;
_audit_update_record             
;
2019-03-07 deposited with the CCDC.	2019-05-17 downloaded from the CCDC.
;

_audit_creation_date             2018-05-04T20:45:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C8 H4 Cu N2 O4 S2, 4(H2 O)'
_chemical_formula_sum            'C8 H12 Cu N2 O8 S2'
_chemical_formula_weight         391.86

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  -P2ybc
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.9681(4)
_cell_length_b                   7.6471(3)
_cell_length_c                   9.1380(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.069(4)
_cell_angle_gamma                90
_cell_volume                     692.66(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    2047
_cell_measurement_theta_min      4.11
_cell_measurement_theta_max      28.752

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       'hexagonal plate // (100), edges {011}, {01-1}'
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             398
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 -1 0.045
1 0 -1 0.035
0 1 -1 0.05
1 -1 -1 0.06
0 0 -1 0.04
0 -1 -1 0.06
-1 0 -1 0.03
-1 -1 -1 0.05
1 1 0 0.055
1 0 0 0.015
1 -1 0 0.065
-1 1 0 0.05
-1 0 0 0.005
-1 -1 0 0.055
1 1 1 0.055
1 0 1 0.035
0 1 1 0.06
0 0 1 0.04
-1 1 1 0.05
0 -1 1 0.06
-1 0 1 0.03
-1 -1 1 0.05

_exptl_crystal_recrystallization_method 
'from solution in water at room temperature,by slow evaporation of solvent'
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
        (compiled Aug  4 2014,14:34:23)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.4372
_exptl_absorpt_correction_T_max  0.9626

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_ambient_temperature      297(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_orient_matrix_ub_11      0.0069007
_diffrn_orient_matrix_ub_12      0.0618237
_diffrn_orient_matrix_ub_13      -0.0565909
_diffrn_orient_matrix_ub_21      0.0708915
_diffrn_orient_matrix_ub_22      -0.0128659
_diffrn_orient_matrix_ub_23      0.0084827
_diffrn_orient_matrix_ub_31      -0.0071736
_diffrn_orient_matrix_ub_32      -0.0678807
_diffrn_orient_matrix_ub_33      -0.0530994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_number            4250
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.48
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_full        26.36
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             1416
_reflns_number_gt                1218
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
        (compiled Aug  4 2014,14:34:23)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
        (compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
        (compiled Aug  4 2014,14:34:23)
;
_computing_structure_solution    'SIR-92 (Altomare et al., 1992)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
;
        ORTEP3 for Windows (Farrugia, 1997)
        MERCURY  (Bruno et al., 2002)
;
_computing_publication_material  
;
        WinGX (Farrugia, 1999)
        PLATON (Spek, 1990-2003)
        enCIFer (Allen et al., 2004)
;

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0364P)²+0.2929P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1416
_refine_ls_number_parameters     113
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0886
_refine_ls_wR_factor_gt          0.0827
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.07

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2422(3) 0.2823(4) -0.0721(3) 0.0404(6) Uani 1 1 d . . .
H1 H 0.1964 0.36 -0.1378 0.048 Uiso 1 1 calc R . .
C2 C 0.3185(3) 0.0452(4) 0.0896(3) 0.0404(7) Uani 1 1 d . . .
H2 H 0.3325 -0.0548 0.1471 0.049 Uiso 1 1 calc R . .
C3 C 0.4079(3) 0.1767(3) 0.0848(3) 0.0328(6) Uani 1 1 d . . .
C4 C 0.5463(3) 0.1991(3) 0.1623(3) 0.0337(6) Uani 1 1 d . . .
N1 N 0.3637(2) 0.3122(3) -0.0076(2) 0.0337(5) Uani 1 1 d . . .
O1 O 0.61085(19) 0.3299(2) 0.1195(2) 0.0366(4) Uani 1 1 d . . .
O2 O 0.5907(2) 0.0949(3) 0.2596(2) 0.0447(5) Uani 1 1 d . . .
S1 S 0.17615(8) 0.08850(10) -0.02448(9) 0.0458(2) Uani 1 1 d . . .
Cu1 Cu 0.5 0.5 0 0.03680(18) Uani 1 2 d S . .
O3 O 0.9579(3) 0.3765(4) 0.1705(3) 0.0657(7) Uani 1 1 d D . .
H3V H 1.016(5) 0.453(6) 0.168(6) 0.15(3) Uiso 1 1 d D . .
H3W H 0.920(3) 0.351(4) 0.091(3) 0.062(12) Uiso 1 1 d D . .
O4 O 0.1374(3) 0.6505(3) 0.1311(3) 0.0522(6) Uani 1 1 d D . .
H4V H 0.215(2) 0.623(5) 0.160(5) 0.091(15) Uiso 1 1 d D . .
H4W H 0.109(5) 0.721(6) 0.193(5) 0.14(2) Uiso 1 1 d D . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.309(3) . ?
C1 S1 1.697(3) . ?
C1 H1 0.93 . ?
C2 C3 1.347(4) . ?
C2 S1 1.702(3) . ?
C2 H2 0.93 . ?
C3 N1 1.379(3) . ?
C3 C4 1.493(4) . ?
C4 O2 1.240(3) . ?
C4 O1 1.274(3) . ?
N1 Cu1 1.974(2) . ?
O1 Cu1 1.9620(18) . ?
Cu1 O1 1.9620(18) 3_665 ?
Cu1 N1 1.974(2) 3_665 ?
O3 H3V 0.825(19) . ?
O3 H3W 0.810(18) . ?
O4 H4V 0.813(19) . ?
O4 H4W 0.845(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 S1 113.7(2) . . ?
N1 C1 H1 123.1 . . ?
S1 C1 H1 123.1 . . ?
C3 C2 S1 110.2(2) . . ?
C3 C2 H2 124.9 . . ?
S1 C2 H2 124.9 . . ?
C2 C3 N1 114.3(2) . . ?
C2 C3 C4 130.6(2) . . ?
N1 C3 C4 115.1(2) . . ?
O2 C4 O1 124.9(2) . . ?
O2 C4 C3 120.6(2) . . ?
O1 C4 C3 114.6(2) . . ?
C1 N1 C3 111.4(2) . . ?
C1 N1 Cu1 138.05(19) . . ?
C3 N1 Cu1 110.53(17) . . ?
C4 O1 Cu1 114.76(16) . . ?
C1 S1 C2 90.35(14) . . ?
O1 Cu1 O1 180 3_665 . ?
O1 Cu1 N1 83.25(8) 3_665 3_665 ?
O1 Cu1 N1 96.75(8) . 3_665 ?
O1 Cu1 N1 96.75(8) 3_665 . ?
O1 Cu1 N1 83.25(8) . . ?
N1 Cu1 N1 180 3_665 . ?
H3V O3 H3W 115(4) . . ?
H4V O4 H4W 108(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3V O4 0.825(19) 1.99(2) 2.804(4) 170(6) 1_655
O3 H3W O4 0.810(18) 2.05(2) 2.826(4) 161(3) 3_665
O4 H4V O2 0.813(19) 2.01(2) 2.820(3) 171(4) 2_655
O4 H4W O3 0.845(19) 1.901(19) 2.746(4) 179(5) 2_655

#----------------------------------------------------------------------------#
#                   SHELXL.RES FILE                                          #
#----------------------------------------------------------------------------#

_iucr_refine_instruction_details 
;
TITL Cu-tha3-a_297K in P2(1)/c
CELL  0.71073   9.9681   7.6471   9.1380   90.000   96.069   90.000
ZERR     2.00   0.0004   0.0003   0.0005    0.000    0.004    0.000
LATT   1
SYMM  - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    N    O    S    CU
UNIT  16   24   4    16   4    2
MERG   2
OMIT     1   1   0
SHEL   13 0.8
DFIX  0.85 O3 H3V O3 H3W O4 H4V O4 H4W
DANG  1.34 H3V H3W H4V H4W
EQIV   $1   x+1,  y,      z
EQIV   $2  -x+1, -y+1,   -z
EQIV   $3  -x+1,  y+1/2, -z+1/2
HTAB     O3  O4_$1
HTAB     O3  O4_$2
HTAB     O4  O2_$3
HTAB     O4  O3_$3
FMAP   2
PLAN   25
SIZE     0.02   0.08   0.14
ACTA
BOND   $H
L.S.   4
TEMP    24.00
WGHT    0.036400    0.292900
FVAR       1.41020
MOLE    1
C1    1    0.242180    0.282280   -0.072053    11.00000    0.03803    0.03997 =
         0.04195    0.00535   -0.00178   -0.00032
AFIX  43
H1    2    0.196351    0.360033   -0.137776    11.00000   -1.20000
AFIX   0
C2    1    0.318494    0.045205    0.089645    11.00000    0.03990    0.03870 =
         0.04094    0.00539   -0.00374   -0.00560
AFIX  43
H2    2    0.332548   -0.054831    0.147097    11.00000   -1.20000
AFIX   0
C3    1    0.407874    0.176705    0.084775    11.00000    0.03278    0.03458 =
         0.03039    0.00044    0.00044   -0.00045
C4    1    0.546292    0.199052    0.162307    11.00000    0.03119    0.03571 =
         0.03362   -0.00320    0.00101    0.00071
N1    3    0.363656    0.312179   -0.007634    11.00000    0.03055    0.03293 =
         0.03674    0.00141   -0.00060   -0.00055
O1    4    0.610846    0.329931    0.119487    11.00000    0.03150    0.03495 =
         0.04218    0.00171   -0.00139   -0.00270
O2    4    0.590659    0.094866    0.259629    11.00000    0.03750    0.05084 =
         0.04383    0.01467   -0.00508   -0.00095
S1    5    0.176152    0.088501   -0.024483    11.00000    0.03650    0.04818 =
         0.05024    0.00624   -0.00650   -0.01026
CU1   6    0.500000    0.500000    0.000000    10.50000    0.03290    0.02996 =
         0.04614    0.00426   -0.00234   -0.00218
MOLE    2
O3    4    0.957902    0.376455    0.170502    11.00000    0.06920    0.07037 =
         0.05464    0.00424   -0.00751   -0.01952
H3V   2    1.015936    0.452989    0.168399    11.00000    0.14661
H3W   2    0.919540    0.350610    0.090808    11.00000    0.06208
MOLE    3
O4    4    0.137439    0.650493    0.131114    11.00000    0.04079    0.06337 =
         0.05061   -0.00575   -0.00326   -0.00091
H4V   2    0.214605    0.623196    0.159854    11.00000    0.09066
H4W   2    0.109378    0.720722    0.192518    11.00000    0.14342
HKLF    4
 
REM  Cu-tha3-a_297K in P2(1)/c
REM R1 =  0.0336 for   1218 Fo > 4sig(Fo)  and  0.0418 for all   1416 data
REM    113 parameters refined using      6 restraints
 
END
 
WGHT      0.0358      0.2876
REM Highest difference peak  0.413,  deepest hole -0.311,  1-sigma level  0.070
Q1    1   0.2214  0.1900 -0.0497  11.00000  0.05    0.41
Q2    1   0.5518  0.3733  0.0223  11.00000  0.05    0.40
Q3    1   0.4304  0.3836 -0.0055  11.00000  0.05    0.38
Q4    1   0.5673  0.4206  0.0960  11.00000  0.05    0.36
Q5    1   0.2507  0.0778  0.0583  11.00000  0.05    0.28
Q6    1   0.3980  0.2357  0.0258  11.00000  0.05    0.27
Q7    1   0.6451  0.1663  0.2637  11.00000  0.05    0.26
Q8    1   0.3169  0.2976 -0.0382  11.00000  0.05    0.25
Q9    1   0.4768  0.1874  0.1315  11.00000  0.05    0.25
Q10   1   0.1601 -0.0858 -0.0287  11.00000  0.05    0.24
Q11   1   0.3749  0.1024  0.0720  11.00000  0.05    0.23
Q12   1   0.6136  0.0639  0.2001  11.00000  0.05    0.23
Q13   1   0.2464  0.0307 -0.0015  11.00000  0.05    0.22
Q14   1   0.1429 -0.0549 -0.0829  11.00000  0.05    0.22
Q15   1   0.9642  0.2869  0.2312  11.00000  0.05    0.21
Q16   1   0.6477  0.2941  0.0432  11.00000  0.05    0.20
Q17   1   0.3356  0.0029  0.0746  11.00000  0.05    0.20
Q18   1   0.1009  0.0133 -0.0349  11.00000  0.05    0.19
Q19   1   0.0581  0.5749  0.1272  11.00000  0.05    0.19
Q20   1   0.2939 -0.1126  0.2605  11.00000  0.05    0.18
Q21   1   0.5633  0.1674  0.2302  11.00000  0.05    0.17
Q22   1   0.5590  0.5273 -0.1117  11.00000  0.05    0.17
Q23   1   0.6627  0.3460  0.1540  11.00000  0.05    0.16
Q24   1   0.9204  0.2217  0.0408  11.00000  0.05    0.16
Q25   1   0.9410  0.3834  0.1263  11.00000  0.05    0.16
;

#----------------------------------------------------------------------------#
#                   VALIDATION RESPONSE FORM                                 #
#----------------------------------------------------------------------------#

# start Validation Reply Form
_vrf_PUBL006_GLOBAL              
;
PROBLEM: _publ_requested_journal is missing
RESPONSE: Not yet submitted
;
_vrf_PUBL012_GLOBAL              
;
PROBLEM: _publ_section_abstract is missing.
RESPONSE: Not yet submitted
;
# end Validation Reply Form

#----------------------------------------------------------------------------#
#                   END OF CIF                                               #
#----------------------------------------------------------------------------#

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
